WO1991017574A1 - Etching indium tin oxide - Google Patents

Etching indium tin oxide Download PDF

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Publication number
WO1991017574A1
WO1991017574A1 PCT/US1991/003065 US9103065W WO9117574A1 WO 1991017574 A1 WO1991017574 A1 WO 1991017574A1 US 9103065 W US9103065 W US 9103065W WO 9117574 A1 WO9117574 A1 WO 9117574A1
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WO
WIPO (PCT)
Prior art keywords
ito
plasma
etching
tin oxide
indium tin
Prior art date
Application number
PCT/US1991/003065
Other languages
French (fr)
Inventor
Paul L. Roselle
Gustavo Roberto Paz-Pujalt
Ronald Myron Wexler
Original Assignee
Eastman Kodak Company
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Eastman Kodak Company filed Critical Eastman Kodak Company
Publication of WO1991017574A1 publication Critical patent/WO1991017574A1/en

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/53—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
    • C04B41/5338—Etching
    • C04B41/5346—Dry etching
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/91—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics involving the removal of part of the materials of the treated articles, e.g. etching
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • H01L31/1884—Manufacture of transparent electrodes, e.g. TCO, ITO
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00844—Uses not provided for elsewhere in C04B2111/00 for electronic applications
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy

Definitions

  • the present invention relates to the etching of indium tin oxide.
  • Solid state CCD image sensors often employ a double polysilicon gate structure to form the sensor electrodes.
  • Such a structure has the first polysilicon electrode (poly-1) separated from the second polysilicon electrode (poly-2) by a thin insulating layer of silicon dioxide.
  • Poly—1 is slightly overlapped by poly—2.
  • the systematic variation of the potential applied to these electrodes referred to as clocking, permits the device to function.
  • clocking permits the device to function.
  • light passes through the polysilicon electrodes and creates electron hole pairs in the underlying silicon. These electrons are accummul ted prior to clocking the polysilicon electrodes to remove the accummulated charge.
  • the polysilicon electrodes, through which light must pass, are not entirely transparent.
  • indium tin oxide would be an effective electrode for such a device.
  • the use of an indium tin oxide electrode enhances the blue response and overall sensitivity of a frame transfer image sensor.
  • the effective ASA of the device could be increased by as much as a factor of two.
  • ITO has not been used on such devices is because it is difficult to pattern such material.
  • the only practical method for etching indium tin oxide has been by immersion in a hot hydroiodic acid solution. Such an acid etches the material isotropically and is not selective to photoresist.
  • ITO can be used as an antistatic coating on materials such as webs used in the manufacture of photosensitive materials. Thereagain, it is difficult to use such a material because it is not practical to pattern it. Disclosure of the Invention
  • a plasma containing methyl radicals (CH 3 ») can effectively etch indium tin oxide anisotropically and with high selectivity to photoresist and silicon dioxide.
  • the above object is achieved in a method of etching indium tin oxide, comprising the steps of: forming a plasma containing CH-*; and etching the ITO by volatilizing the ITO by a reaction with the plasma of CH 3 «.
  • FIG. la is a schematic, in partial cross—section, of a conventional plasma etcher which uses radio frequency energy to ignite and sustain the plasma.
  • FIG. 2 is a schematic, in partial cross—section, of another plasma etcher which uses microwave energy to ignite and sustain the plasma.
  • FIG. 3 shows various steps in patterning an ITO layer formed on an Si0 2 insulating layer provided on a silicon substrate.
  • a plasma is a state of matter in which the gases in a vessel with a total pressure less than atmospheric pressure are partially ionized by an electric field.
  • an electric field can be from a radio frequency generator, microwave frequency generator or DC voltage field.
  • a plasma ignited by the action of such an electric field on a mixture of CH, gas and H 2 gas, will contain methyl radicals (CH- as well as other species generated from the cracking of the molecules of CH, and H 2 .
  • CH, and H 2 mixtures are not the only means of producing methyl radicals (CH.,*) and that mixtures of ethane and hydrogen, propane and hydrogen, or other organic compounds will result in methyl radical creation in plasma and will, in so doing, etch ITO.
  • a wafer 18 is placed on a lower electrode 15 which is connected to an RF radiation source 28. Vacuum is achieved in the chamber by the use of an oil diffusion pump and rotary vacuum pump, not shown.
  • the lower electrode 15 is heated by resistive heaters 16 located on the back of the electrode.
  • the H 2 and CH, gases are admitted into the chamber through a diffuser 26.
  • the flows of the gases are regulated by mass flow controllers 22 and 24.
  • Process pressure in the vessel is controlled by a vacuum throttle valve 21. When the desired flow rates, pressure and temperature are achieved, a plasma of CH, and H 2 is ignited in a space 30 between the lower electrode 15, on which the wafer 18 sits, and an upper electrode 12.
  • the resultant CH 3 » generated in region 30 will react with the ITO on the wafer 18 volatilizing the ITO off the wafer to be pumped away by the vacuum pump.
  • the pressure of the plasma of CH, and H 2 must be maintained below the polymerization point of the plasma.
  • the ratio of CH ⁇ to H 2 should be less than 20% to prevent excessive polymerization of the species in the plasma. Such excessive polymerization produced by too high of a pressure and/or too high of a concentration of CH ⁇ . in H 2 will prevent ITO from etching.
  • the source of the plasma excitation is a microwave generator 10 located on top of the vacuum chamber.
  • a wafer 20 is placed on a lower electrode 19 which can be biased by an additional power source if needed.
  • Vacuum is achieved with a vacuum pump (not shown) .
  • H 2 and CH ⁇ . gases are admitted into the plasma generation region 17.
  • the flows of the gases are controlled by mass flow controllers 12 and 14 and the pressure in the chamber is maintained by a throttle valve 25.
  • the microwave energy is sent into the plasma generating region 17 through a wave guide 11 where it partially ionizes the gases into a plasma state.
  • the CH 3 » species generated in this plasma travel to the wafer 20 and etch the exposed ITO off of the wafer.
  • FIGS. 3a-c show the process of pattern transfer for the definition of ITO where the etched ITO is to be used as a poly-1 electrode.
  • microlithographic photoresist mask 34 has been deposited and patterned in a conventional manner on the surface of an ITO layer 32 which has been deposited on an Si0 2 layer 30 on a silicon substrate 36.
  • ITO is most usually deposited by RF sputter deposition.
  • the ITO layer 32 has been etched anisotropically by the plasma of CH 3 » thereby transferring the photoresist pattern into the ITO and stopping on the Si0 2 layer 30. Measurements have shown that the plasma of CH.-,* that etches the ITO has a high selectivity to both the photoresist and the underlying Si0 2 layer.
  • the photoresist 34 has been stripped off of the ITO 32 and the device may proceed to further processing.
  • the photoresist is most usually removed by 0 2 plasma stripping.
  • the mechanism of etching of ITO is believed to be caused by methyl radicals reacting with indium and tin to create volatile organometallic compounds as shown by the following reaction: plasma CH 4 +H 2 >CH 3 -+In+Sn+0 ⁇ -In(CH 3 ) 3 t+Sn(CH 3 ) t+COt ITO
  • An etcher similar to the one represented by FIG. 1 was used to etch ITO.
  • the radio frequency used to ignite and sustain the plasma was 13.56 megahertz at 85 watts forward power.
  • the wafer was heated to a temperature of 70°C.
  • the chamber was evacuated to a base pressure of 1 x 10 ⁇ prior to the admission of the CH, and H 2 gases.
  • the flow rate for the CH ⁇ was 25 seem and the flow rate the the ⁇ 2 was 150 seem.
  • a process pressure of 150 Mtorr was maintained during the etch.

Abstract

ITO is etched by a plasma containing CH3. gas.

Description

ETCHING INDIUM TIN OXIDE Technical Field
The present invention relates to the etching of indium tin oxide. Background Art
Solid state CCD image sensors often employ a double polysilicon gate structure to form the sensor electrodes. Such a structure has the first polysilicon electrode (poly-1) separated from the second polysilicon electrode (poly-2) by a thin insulating layer of silicon dioxide. Poly—1 is slightly overlapped by poly—2. The systematic variation of the potential applied to these electrodes, referred to as clocking, permits the device to function. In the case of frame transfer CCD image sensors, light passes through the polysilicon electrodes and creates electron hole pairs in the underlying silicon. These electrons are accummul ted prior to clocking the polysilicon electrodes to remove the accummulated charge. The polysilicon electrodes, through which light must pass, are not entirely transparent. This lack of transparency results in the reduction of sensitivity and spectral response of the image sensor. Due to its transparency, it has been recognized that indium tin oxide would be an effective electrode for such a device. The use of an indium tin oxide electrode enhances the blue response and overall sensitivity of a frame transfer image sensor. In fact, it has been recognized that if indium tin oxide were to be used in such a device the effective ASA of the device could be increased by as much as a factor of two. One reason that ITO has not been used on such devices is because it is difficult to pattern such material. Heretofore, the only practical method for etching indium tin oxide has been by immersion in a hot hydroiodic acid solution. Such an acid etches the material isotropically and is not selective to photoresist. These two reasons alone show the difficulties involved in using ITO for microelectronic applications where small features are defined by photoresist lithography.
It has also been recognized that ITO can be used as an antistatic coating on materials such as webs used in the manufacture of photosensitive materials. Thereagain, it is difficult to use such a material because it is not practical to pattern it. Disclosure of the Invention
It is the object of this invention to provide a new method for the etching of indium tin oxide. In accordance with this invention, it has been discovered that a plasma containing methyl radicals (CH3») can effectively etch indium tin oxide anisotropically and with high selectivity to photoresist and silicon dioxide. The above object is achieved in a method of etching indium tin oxide, comprising the steps of: forming a plasma containing CH-*; and etching the ITO by volatilizing the ITO by a reaction with the plasma of CH3«. Brief Description of the Drawings
FIG. la is a schematic, in partial cross—section, of a conventional plasma etcher which uses radio frequency energy to ignite and sustain the plasma. FIG. 2 is a schematic, in partial cross—section, of another plasma etcher which uses microwave energy to ignite and sustain the plasma.
FIG. 3 shows various steps in patterning an ITO layer formed on an Si02 insulating layer provided on a silicon substrate. Mode of Carrying Out the Invention
With reference to FIGS. 1, 2 and 3a-3c, a process for the plasma etching of indium tin oxide is described. A plasma is a state of matter in which the gases in a vessel with a total pressure less than atmospheric pressure are partially ionized by an electric field. As is well understood, such an electric field can be from a radio frequency generator, microwave frequency generator or DC voltage field.
A plasma, ignited by the action of such an electric field on a mixture of CH, gas and H2 gas, will contain methyl radicals (CH- as well as other species generated from the cracking of the molecules of CH, and H2. As in any plasma, the concentrations of the various species in the plasma depend upon the power and frequency of the electric field applied, the pressure of the plasma, and the concentrations of the gases used. It should be understood that CH, and H2 mixtures are not the only means of producing methyl radicals (CH.,*) and that mixtures of ethane and hydrogen, propane and hydrogen, or other organic compounds will result in methyl radical creation in plasma and will, in so doing, etch ITO.
For an etcher as represented in FIG. 1, a wafer 18 is placed on a lower electrode 15 which is connected to an RF radiation source 28. Vacuum is achieved in the chamber by the use of an oil diffusion pump and rotary vacuum pump, not shown. The lower electrode 15 is heated by resistive heaters 16 located on the back of the electrode. The H2 and CH, gases are admitted into the chamber through a diffuser 26. The flows of the gases are regulated by mass flow controllers 22 and 24. Process pressure in the vessel is controlled by a vacuum throttle valve 21. When the desired flow rates, pressure and temperature are achieved, a plasma of CH, and H2 is ignited in a space 30 between the lower electrode 15, on which the wafer 18 sits, and an upper electrode 12. The resultant CH3» generated in region 30 will react with the ITO on the wafer 18 volatilizing the ITO off the wafer to be pumped away by the vacuum pump. The pressure of the plasma of CH, and H2 must be maintained below the polymerization point of the plasma. Likewise, the ratio of CH^ to H2 should be less than 20% to prevent excessive polymerization of the species in the plasma. Such excessive polymerization produced by too high of a pressure and/or too high of a concentration of CH^. in H2 will prevent ITO from etching.
For an etcher system as represented in FIG. 2, the source of the plasma excitation is a microwave generator 10 located on top of the vacuum chamber. A wafer 20 is placed on a lower electrode 19 which can be biased by an additional power source if needed. Vacuum is achieved with a vacuum pump (not shown) . H2 and CH^. gases are admitted into the plasma generation region 17. The flows of the gases are controlled by mass flow controllers 12 and 14 and the pressure in the chamber is maintained by a throttle valve 25. When the plasma is to be ignited the microwave energy is sent into the plasma generating region 17 through a wave guide 11 where it partially ionizes the gases into a plasma state. The CH3» species generated in this plasma travel to the wafer 20 and etch the exposed ITO off of the wafer.
FIGS. 3a-c show the process of pattern transfer for the definition of ITO where the etched ITO is to be used as a poly-1 electrode. In FIG. 3a it is seen that microlithographic photoresist mask 34 has been deposited and patterned in a conventional manner on the surface of an ITO layer 32 which has been deposited on an Si02 layer 30 on a silicon substrate 36. ITO is most usually deposited by RF sputter deposition.
In FIG. 3b the ITO layer 32 has been etched anisotropically by the plasma of CH3» thereby transferring the photoresist pattern into the ITO and stopping on the Si02 layer 30. Measurements have shown that the plasma of CH.-,* that etches the ITO has a high selectivity to both the photoresist and the underlying Si02 layer.
In FIG. 3c the photoresist 34 has been stripped off of the ITO 32 and the device may proceed to further processing. The photoresist is most usually removed by 02 plasma stripping. Example
Without limiting the generality of this invention, the mechanism of etching of ITO is believed to be caused by methyl radicals reacting with indium and tin to create volatile organometallic compounds as shown by the following reaction: plasma CH4+H2 >CH3-+In+Sn+0→-In(CH3)3t+Sn(CH3) t+COt ITO
Other starting gases can be used provided they form a plasma having CH3«.
An etcher similar to the one represented by FIG. 1 was used to etch ITO. The radio frequency used to ignite and sustain the plasma was 13.56 megahertz at 85 watts forward power. The wafer was heated to a temperature of 70°C. The chamber was evacuated to a base pressure of 1 x 10~ prior to the admission of the CH, and H2 gases. The flow rate for the CH^ was 25 seem and the flow rate the the Ξ2 was 150 seem. A process pressure of 150 Mtorr was maintained during the etch. The sputter deposited ITO etched at a rate of 275 angstroms per minute and showed very high selectivity to the photoresist and the underlying silicon dioxide: Cross—sectional scanning electron micrographs of the etched ITO showed the etch to be highly anisotropic with no evidence of undercutting the photoresist.
The invention has been described in detail with particular reference to certain preferred embodiments thereof, but it will be understood that variations and modifications can be effected within the spirit and scope of the invention.

Claims

CLAIMS :
1. A method of etching ITO comprising the steps of: forming a plasma containing CH3»; and • etching the ITO by volatilizing ITO by reacting ITO with the plasma generated CH.,*.
2. A method according to claim 1 wherein the plasma is formed from a gas mixture of CH, and H2.
3. A method of etching ITO on a substrate comprising the steps of:
(a) depositing and patterning a microlithographic mask on the ITO surface to expose portions of the ITO; and (b) igniting a plasma containing CH.-,* which etch the exposed ITO portions thereby transferring the pattern into the ITO, anisotropically.
4. A method according to claim 3 wherein said substrate is a silicon substrate covered with a
Si02 layer and wherein said plasma is formed from a gas mixture of CH, and H2.
5. The method of claim 3 wherein the plasma is formed by mixing CH, gas and Ξ2 gas in a chamber at a pressure selected to prevent polymerization; and igniting a plasma of the CH, and H2 by subjecting the mixture to RF or microwave radiation or other suitable electric field.
6. The method of claim 5 wherein the ratio CH to H is less than 207-.
PCT/US1991/003065 1990-05-07 1991-05-03 Etching indium tin oxide WO1991017574A1 (en)

Applications Claiming Priority (2)

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US520,486 1990-05-07
US07/520,486 US5032221A (en) 1990-05-07 1990-05-07 Etching indium tin oxide

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US5171401A (en) * 1990-06-04 1992-12-15 Eastman Kodak Company Plasma etching indium tin oxide
US5318664A (en) * 1990-06-25 1994-06-07 General Electric Company Patterning of indium-tin oxide via selective reactive ion etching
US5230771A (en) * 1991-04-08 1993-07-27 Eastman Kodak Company Plasma etching indium tin oxide using a deposited silicon nitride mask
US5286337A (en) * 1993-01-25 1994-02-15 North American Philips Corporation Reactive ion etching or indium tin oxide
US5340438A (en) * 1993-06-07 1994-08-23 Eastman Kodak Company Low temperature insitu image reversal process for microelectric fabrication
US5292682A (en) * 1993-07-06 1994-03-08 Eastman Kodak Company Method of making two-phase charge coupled device
EP0652585A1 (en) * 1993-11-02 1995-05-10 Leybold Aktiengesellschaft Process and device for etching thin layers, preferably Indium-Tin-Oxide layers
US5468296A (en) * 1993-12-17 1995-11-21 Lsi Logic Corporation Apparatus for igniting low pressure inductively coupled plasma
US5696428A (en) * 1995-06-07 1997-12-09 Lsi Logic Corporation Apparatus and method using optical energy for specifying and quantitatively controlling chemically-reactive components of semiconductor processing plasma etching gas
US5843277A (en) * 1995-12-22 1998-12-01 Applied Komatsu Technology, Inc. Dry-etch of indium and tin oxides with C2H5I gas
KR100468700B1 (en) * 1997-12-30 2005-03-16 삼성전자주식회사 Dry etching process for forming fine pattern of semiconduct of device
US6544367B1 (en) * 1999-02-01 2003-04-08 Alliant Techsystems Inc. Overwrap tape end-effector for fiber placement/winding machines
US6275277B1 (en) 1999-05-17 2001-08-14 Colorado Microdisplay, Inc. Micro liquid crystal displays having a circular cover glass and a viewing area free of spacers
US8050486B2 (en) * 2006-05-16 2011-11-01 The Boeing Company System and method for identifying a feature of a workpiece
JP6004420B2 (en) * 2012-03-14 2016-10-05 国立研究開発法人産業技術総合研究所 Method for removing non-volatile compounds
US9824893B1 (en) 2016-06-28 2017-11-21 Lam Research Corporation Tin oxide thin film spacers in semiconductor device manufacturing
KR20180093798A (en) 2017-02-13 2018-08-22 램 리써치 코포레이션 Method to create air gaps
US10546748B2 (en) 2017-02-17 2020-01-28 Lam Research Corporation Tin oxide films in semiconductor device manufacturing
KR102630349B1 (en) 2018-01-30 2024-01-29 램 리써치 코포레이션 Tin oxide mandrels in patterning
US10840082B2 (en) * 2018-08-09 2020-11-17 Lam Research Corporation Method to clean SnO2 film from chamber
JP7320085B2 (en) 2019-06-27 2023-08-02 ラム リサーチ コーポレーション Alternating etching and passivation processes
CN113451473A (en) * 2020-07-07 2021-09-28 重庆康佳光电技术研究院有限公司 Etching method of indium tin oxide layer and manufacturing method of chip

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US5032221A (en) 1991-07-16
JPH04506888A (en) 1992-11-26
EP0483319A1 (en) 1992-05-06

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